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In vitro, hydrogel-based ECMs for functionalizing surfaces of various material have played an essential role in mimicking native tissue matrix. Polydimethylsiloxane (PDMS) is widely used to build microfluidic or organ-on-chip devices compatible with cells due to its easy handling in cast replication. Despite such advantages, the limitation of PDMS is its hydrophobic surface property. To improve wettability of PDMS-based devices, alginate, a naturally derived polysaccharide, was covalently bound to the PDMS surface. This alginate then crosslinked further hydrogel onto the PDMS surface in desired layer thickness. Hydrogel-modified PDMS was used for coating a topography chip system and in vitro investigation of cell growth on the surfaces. Moreover, such hydrophilic hydrogel-coated PDMS is utilized in a microfluidic device to prevent unspecific absorption of organic solutions. Hence, in both exemplary studies, PDMS surface properties were modified leading to improved devices.
Palladium-doped silica materials with SiCH3 groups were fabricated by sol-gel method under various calcination atmospheres and membranes were made thereof by coating process. The results showed that air atmosphere can lead to the partial oxidation of metallic Pd0 to PdO while N2 and H2 atmospheres can effectively prevent metallic Pd0 from being oxidized. H2 atmosphere is proved to be a more prominent way to slow down the decomposition of organic SiCH3 group than N2 and air atmospheres. The surface area, micropore volume and porosity of palladium-doped silica membrane material calcined in H2 atmosphere are much higher than those calcined in N2 atmosphere. Compared with N2 atmosphere, the palladium-doped silica membranes calcined in H2 atmosphere showed higher H2 permeability and H2/CO2 selectivity before and after the steam exposure. The apparent activation energy of H2 permeation through the palladium-doped silica membrane calcined under H2 atmosphere (2.51 ± 0.05 kJ/mol) was slightly lower than that calcined under N2 atmosphere (2.84 ± 0.04 kJ/mol). Calcination atmosphere plays some role in membrane performance, which has greater influence on the permeance than on the gas permselectivity. Calcination under H2 atmosphere is well conducive to improve the gas permeance and H2 permselectivity of palladium-doped silica membrane.
Purpose: Human breath analysis is proposed with increasing frequency as a useful tool in clinical application. We performed this study to find the characteristic volatile organic compounds (VOCs) in the exhaled breath of patients with idiopathic pulmonary fibrosis (IPF) for discrimination from healthy subjects. Methods: VOCs in the exhaled breath of 40 IPF patients and 55 healthy controls were measured using a multi-capillary column and ion mobility spectrometer. The patients were examined by pulmonary function tests, blood gas analysis, and serum biomarkers of interstitial pneumonia. Results: We detected 85 VOC peaks in the exhaled breath of IPF patients and controls. IPF patients showed 5 significant VOC peaks; p-cymene, acetoin, isoprene, ethylbenzene, and an unknown compound. The VOC peak of p-cymene was significantly lower (p < 0.001), while the VOC peaks of acetoin, isoprene, ethylbenzene, and the unknown compound were significantly higher (p < 0.001 for all) compared with the peaks of controls. Comparing VOC peaks with clinical parameters, negative correlations with VC (r =−0.393, p = 0.013), %VC (r =−0.569, p < 0.001), FVC (r = −0.440, p = 0.004), %FVC (r =−0.539, p < 0.001), DLco (r =−0.394, p = 0.018), and %DLco (r =−0.413, p = 0.008) and a positive correlation with KL-6 (r = 0.432, p = 0.005) were found for p-cymene. Conclusion: We found characteristic 5 VOCs in the exhaled breath of IPF patients. Among them, the VOC peaks of p-cymene were related to the clinical parameters of IPF. These VOCs may be useful biomarkers of IPF.
This review gives a short overview of the physical processes involved in the formation of the polyelectrolyte multilayers (PEMs) and their destruction. These two processes are vital for the formation of PEMs with desired physical and chemical structures, and for loading them with active substances and their spatial controlled release. It includes a survey of the physical and chemical properties that are key points for controlling film nanostructure in relation to biological processes and different possibilities for controlling cell behavior by means of film composition, bioactivity, mechanical properties, and three-dimensional organization.
Here, we report the mechanical and water sorption properties of a green composite based on Typha latifolia fibres. The composite was prepared either completely binder-less or bonded with 10% (w/w) of a bio-based resin which was a mixture of an epoxidized linseed oil and a tall-oil based polyamide. The flexural modulus of elasticity, the flexural strength and the water absorption of hot pressed Typha panels were measured and the influence of pressing time and panel density on these properties was investigated. The cure kinetics of the biobased resin was analyzed by differential scanning calorimetry (DSC) in combination with the iso-conversional kinetic analysis method of Vyazovkin to derive the curing conditions required for achieving completely cured resin. For the binderless Typha panels the best technological properties were achieved for panels with high density. By adding 10% of the binder resin the flexural strength and especially the water absorption were improved significantly.
Powder coating of engineered wood panels such as medium density fibreboards (MDF) is gaining industrial interest due to ecological and economic advantages of powder coating technology. For transferring powder coating technology to temperature-sensitive substrates like MDF, a thorough understanding of the melting, flowing and curing behaviour of the used low-bake resins is required. In the present study, thermo-analysis in combination with iso-conversional kinetic data analysis as well as rheometry is applied to characterise the properties of an epoxy-based powder coating. Neat resin and cured powder coating films are examined in order to define an ideal production window within which the resin is preferably applied and processed to yield satisfactory surface performance on the one hand and without exposing the carrier MDF too high a temperature load on the other hand to prevent the panel from deteriorating in mechanical strength. In order to produce powder coated films of high surface gloss – a feature that has not yet successfully been realized on MDF with powder coatings – a new curing technology, in-mould surface finishing, has been applied.
Within the scope of the present cumulative doctoral thesis six scientific papers were published which illustrates that modern reaction model-free (=isoconversional) kinetic analysis (ICKA) methods represents a universal and effective tool for the controlled processing of thermosetting materials. In order to demonstrate the universal applicability of ICKA methods, the thermal cure of different thermosetting materials having a very broad range of chemical composition (melamine-formaldehyde resins, epoxy resins, polyester-epoxy resins, and acrylate/epoxy resins) were analyzed and mathematically modelled. Some of the materials were based on renewable resources (an epoxy resin was made from hempseed oil; linseed oil was modified into an acrylate/epoxy resin). With the aid of ICKA methods not only single-step but also complex multi-step reactions were modelled precisely. The analyzed thermosetting materials were combined with wood, wood-based products, paper, and plant fibers which are processed to various final products. Some of the thermosetting materials were applied as coating (in form of impregnated décor papers or powder and wet coatings respectively) on wood substrates and the epoxy resin from hempseed oil was mixed with plant fibers and processed into bio-based composites for lightweight applications. From the final products mechanical, thermal, and surface properties were determined. The activation energy as function of cure conversion derived from ICKA methods was utilized to predict accurately the thermal curing over the course of time for arbitrary cure conditions. Furthermore the cure models were used to establish correlations between the cross-linking during processing into products and the properties of the final products. Therewith it was possible to derive the process time and temperature that guarantee optimal cross-linking as well as optimal product properties
The world population is growing and alternative ways of satisfying the increasing demand for meat are being explored, such as using animal cells for the fabrication of cultured meat. Edible biomaterials are required as supporting structures. Hence, we chose agarose, gellan and a xanthan-locust bean gum blend (XLB) as support materials with pea and soy protein additives and analyzed them regarding material properties and biocompatibility. We successfully built stable hydrogels containing up to 1% pea or soy protein. Higher amounts of protein resulted in poor handling properties and unstable gels. The gelation temperature range for agarose and gellan blends is between 23–30 °C, but for XLB blends it is above 55 °C. A change in viscosity and a decrease in the swelling behavior was observed in the polysaccharide-protein gels compared to the pure polysaccharide gels. None of the leachates of the investigated materials had cytotoxic effects on the myoblast cell line C2C12. All polysaccharide-protein blends evaluated turned out as potential candidates for cultured meat. For cell-laden gels, the gellan blends were the most suitable in terms of processing and uniform distribution of cells, followed by agarose blends, whereas no stable cell-laden gels could be formed with XLB blends.
Rats are commonly used in medical research as they enable a high grade of standardization. The exhalome of ventilated rats has not as yet been investigated using an ion mobility spectrometer coupled with a multi-capillary column (MCC-IMS). As a first step, a rat model has to be established to measure potential biomarkers in the exhale with long-term settings, allowing constant and continuous analysis of exhaled air in time series. Therefore, eight animals were anaesthetized, prepared and ventilated for 1 h. A total of 73 peaks were directly detected with the IMS chromatogram. Thirty five of them were assigned to the ventilator system and 38 to the animals. Peak intensity varied within three measurements. The intensity of analytes of individual rats varied by a factor of up to 18. This new model will also enable continuous measurements of volatile organic compounds (VOCs) from rat's breath in long-term experiments. It is hoped that, in the future, variability and progression of VOCs can be monitored in different models of diseases using this set-up.
Hardboards (HBs) (wet-process high-density fibreboards) were made in an industrial trial using a binder system consisting of cationic mimosa tannin and laccase or just cationic tannin without any thermosetting adhesive. The boards displayed superior mechanical strength compared to reference boards made with phenol–formaldehyde, easily exceeding the European standards for general-purpose HBs. The thickness swell of most of the boards was slightly greater than the standards would allow, so some optimisation is required in this area. The improved board properties appear to be mainly associated with ionic interactions involving quaternary amino groups in cationic tannin and negatively charged wood fibres rather than to cross-linking of fibres via laccase-assisted formation and coupling of radicals in tannin and fibre lignin.
Exogenous factors of influence on exhaled breath analysis by ion-mobility spectrometry (MCC/IMS)
(2019)
The interpretation of exhaled breath analysis needs to address to the influence of exogenous factors, especially to a transfer of confounding analytes by the test persons. A test person who was exposed to a disinfectant had exhaled breath analysis by MCC/IMS (Bioscout®) after different time intervals. Additionally, a new sampling method with inhalation of synthetic air before breath analysis was tested. After exposure to the disinfectant, 3-Pentanone monomer, 3-Pentanone dimer, Hexanal, 3-Pentanone trimer, 2-Propanamine, 1-Propanol, Benzene, Nonanal showed significantly higher intensities, in exhaled breath and air of the examination room, compared to the corresponding baseline measurements. Only one ingredient of the disinfectant (1-Propanol) was identical to the 8 analytes. Prolonging the time intervals between exposure and breath analysis showed a decrease of their intensities. However, the half-time of the decrease was different. The inhalation of synthetic air - more than consequently airing the examination room with fresh air - reduced the exogenous and also relevant endogenous analytes, leading to a reduction and even changing polarity of the alveolar gradient. The interpretation of exhaled breath needs further knowledge about the former residence of the proband and the likelihood and relevance of the inhalation of local, site-specific and confounding exogenous analytes by him. Their inhalation facilitates a transfer to the examination room and a detection of high concentrations in room air and exhaled breath, but also the exhalation of new analytes. This may lead to a misinterpretation of these analytes as endogenous resp. disease-specific ones.
Standardisation of breath sampling is important for application of breath analysis in clinical settings. By studying the effect of room airing on indoor and breath analytes and by generating time series of room air with different sampling intervals we sought to get further insights into room air metabolism, to detect the relevance of exogenous VOCs and to make conclusions about their consideration for the interpretation of exhaled breath. Room air and exhaled breath of a healthy subject were analysed before and after room airing. Furthermore a time series of room air with doors and windows closed was taken over 84 h by an automatic sampling every 180 min. A second times series studied room air analytes over 70 h with samples taken every 16.5 min. For breath and room air measurements an IMS coupled to a multi-capillary column (IMS/MCC) [Bio-Scout® - B&S Analytik GmbH, Dortmund, Germany] was used. The peaks were characterized using the Software Visual Now (B&S Analytik, Dortmund Germany) and identified using the software package MIMA (version 1.1, provided by the Max Planck Institute for Informatics, Saarbrücken, Germany) and the database 20160426_SubstanzDbNIST_122 (B & S Analytik GmbH, Dortmund, Germany). In the morning 4 analytes (Decamethylcylopentasiloxane [541-02-6]; Pentan-2-one [107-87-9] – Dimer; Hexan-1-al [66-25-1]; Pentan-2-one [107-87-9]) – Monomer showed high intensities in the room air and exhaled breath. They were significantly but not equally reduced by room airing. The time series about 84 h showed a time dependent decrease of analytes (limonen-monomer and -dimer; Decamethylcylopentasiloxane, Butan-1-ol, Butan-1-ol) as well as increase (Pentan-2-one [107-87-9] – Dimer). Shorter sampling intervals exhibited circadian variations of analyte concentrations for many analytes. Breath sampling in the morning needs room airing before starting. Then the variation of the intensity of indoor analytes can be kept small. The time series of indoor analytes show, that their intensities have a different behaviour, with time dependent declines, constant increases and circadian variations, dependent on room airing. This has implications on the breath sampling procedure and the intrepretation of exhaled breath.
The coculture of osteogenic and angiogenic cells and the resulting paracrine signaling via soluble factors are supposed to be crucial for successfully engineering vascularized bone tissue equivalents. In this study, a coculture system combining primary human adiposederived stem cells (hASCs) and primary human dermal microvascular endothelial cells (HDMECs) within two types of hydrogels based on methacryloyl‐modified gelatin (GM) as three‐dimensional scaffolds was examined for its support of tissue specific cell functions. HDMECs, together with hASCs as supporting cells, were encapsulated in soft GM gels and were indirectly cocultured with hASCs encapsulated in stiffer GM hydrogels additionally containing methacrylate‐modified hyaluronic acid and hydroxyapatite particles. After 14 days, the hASC in the stiffer gels (constituting the “bone gels”) expressed matrix proteins like collagen type I and fibronectin, as well as bone‐specific proteins osteopontin and alkaline phosphatase. After 14 days of coculture with HDMEC‐laden hydrogels, the viscoelastic properties of the bone gels were significantly higher compared with the gels in monoculture. Within the soft vascularization gels, the formed capillary‐like networks were significantly longer after 14 days of coculture than the structures in the control gels. In addition, the stability as well as the complexity of the vascular networks was significantly increased by coculture. We discussed and concluded that osteogenic and angiogenic signals from the culture media as well as from cocultured cell types, and tissue‐specific hydrogel composition all contribute to stimulate the interplay between osteogenesis and angiogenesis in vitro and are a basis for engineering vascularized bone.
In bioprinting approaches, the choice of bioink plays an important role since it must be processable with the selected printing method, but also cytocompatible and biofunctional. Therefore, a crosslinkable gelatin-based ink was modified with hydroxyapatite (HAp) particles, representing the composite buildup of natural bone. The inks’ viscosity was significantly increased by the addition of HAp, making the material processable with extrusion-based methods. The storage moduli of the formed hydrogels rose significantly, depicting improved mechanical properties. A cytocompatibility assay revealed suitable ranges for photoinitiator and HAp concentrations. As a proof of concept, the modified ink was printed together with cells, yielding stable three-dimensional constructs containing a homogeneously distributed mineralization and viable cells.
Though bioprinting is a forward-looking approach in bone tissue engineering, the development of bioinks which are on the one hand processable with the chosen printing technique, and on the other hand possess the relevant mechanical as well as osteoconductive features remains a challenge. In the present study, polymer solutions based on methacrylated gelatin and methacrylated hyaluronic acid modified with hydroxyapatite (HAp) particles (5 wt%) were prepared. Encapsulation of primary human adipose derived stem cells in the HAp-containing gels and culture for 28 d resulted in a storage moduli significantly increased to 126% ± 9.6% compared to the value on day 1 by the sole influence of the HAp. Additional use of osteogenic media components resulted in an increase of storage module up to 199% ± 27.8%. Similarly, the loss moduli was increased to 370% ± 122.1% under the influence of osteogenic media components and HAp. Those changes in rheological material characteristics indicate a distinct change in elastic and viscous hydrogel properties, and are attributed to extensive matrix production in the hydrogels by the encapsulated cells, what could also be proven by staining of bone matrix components like collagen I, fibronectin, alkaline phosphatase and osteopontin. When using the cell-laden polymer solutions as bioinks to build up relevant geometries, the ink showed excellent printability and the printed grid structure's integrity remained intact over a culture time of 28 d. Again, an intense matrix formation as well as upregulation of osteogenic markers by the encapsulated cells could be shown. In conclusion, we demonstrated that our HAp-containing bioinks and hydrogels on basis of methacrylated gelatin and hyaluronic acid are on the one hand highly suitable for the build up of relevant three-dimensional geometries with microextrusion bioprinting, and on the other hand exhibit a significant positive effect on bone matrix development and remodeling in the hydrogels, as indicated by rheological measurements and staining of bone components. This makes the developed composite hydrogels an excellent material for bone bioprinting approaches.
Melamine–formaldehyde (MF) resins are widely used as adhesives and finishing materials in the wood industry. During resin cure, either methylene ether or methylene bridges are formed, leading to the formation of a three‐dimensional resin network. Not only the curing degree, but also the chemical species present in the cured resin determine the quality of the final product. Analytical methods allowing a detailed investigation of network formation are of great benefit to manufacturers. In the present work, resin cure of an MF precondensate is studied at different temperatures (100–200 °C) without considering the initial pH as a factor. Isoconversional kinetic analysis based on exothermal curing enthalpies enables calculation of the crosslinking degree at a given time/temperature regime. A semiquantitative determination of the chemical groups present is performed based on solid‐state nuclear magnetic resonance data. Fourier transform infrared spectroscopy has shown to be a fast and reliable analytical tool with high sensitivity toward functional groups and with great potential for at‐line process control.
The isothermal curing of melamine resin is investigated by in-line infrared spectroscopy at different temperatures. The infrared spectra are decomposed into time courses of characteristic spectral patterns using Multivariate Curve Resolution (MCR). It was found that depending on the applied curing temperature, melamine films with different spectral fingerprints and correspondingly different chemical network structures are formed. The network structures of fully cured resin films are specific for the applied curing temperatures used and cannot simply be compensated by changes in the curing time. For industrial curing processes, this means that cure temperature is the main system determining factor at constant M:F ratio. However, different MF resin networks can be specifically obtained from one and the same melamine resin by suitable selection of the curing time and temperatures profiles to design resin functionality. The spectral fingerprints after short curing time as well as after long curing time reflect the fundamental differences in the thermoset networks that can be obtained with industrial short-cycle and multi-daylight presses.
Here, we study resin cure and network formation of solid melamine formaldehyde pre-polymer over a large temperature range viadynamic temperature curing profiles. Real-time infrared spectroscopy is used to analyze the chemical changes during network formation and network hardening. By applying chemometrics (multivariate curve resolution,MCR), the essential chemical functionalities that constitute the network at a given stage of curing are mathematically extracted and tracked over time. The three spectral components identified by MCR were methylol-rich, ether linkages-rich and methylene linkages-rich resin entities. Based on dynamic changes of their characteristic spectral patterns in dependence of temperature, curing is divided into five phases: (I) stationary phase with free methylols as main chemical feature, (II) formation of flexible network cross-linked by ether linkages, (III) formation of rigid, ether-cross-linked network, (IV) further hardening via transformation of methylols and ethers into methylene-cross-linkages, and (V) network consolidation via transformation of ether into methylene bridges. The presented spectroscopic/chemometric approach can be used as methodological basis for the functionality design of MF-based surface films at the stage of laminate pressing, i.e., for tailoring the technological property profile of cured MF films using a causal understanding of the underlying chemistry based on molecular markers and spectroscopic fingerprints.
During curing of thermosetting resins the technologically relevant properties of binders and coatings develop. However, curing is difficult to monitor due to the multitude of chemical and physical processes taking place. Precise prediction of specific technological properties based on molecular properties is very difficult. In this study, the potential of principal component analysis (PCA) and principal component regression (PCR) in the analysis of Fourier transform infrared (FTIR) spectra is demonstrated using the example of melamine-formaldehyde (MF) resin curing in solid state. FTIR/PCA-based reaction trajectories are used to visualize the influence of temperature on isothermal cure. An FTIR/PCR model for predicting the hydrolysis resistance of cured MF resin from their spectral fingerprints is presented which illustrates the advantages of FTIR/PCR compared to the combination differential scanning calorimetry/isoconversional kinetic analysis. The presented methodology is transferable to the curing reactions of any thermosetting resin and can be applied to model other technologically relevant final properties as well.